scholarly journals Multiresidue Method for the Determination of Residues of 251 Pesticides in Fruits and Vegetables by Gas Chromatography/Mass Spectrometry and Liquid Chromatography with Fluorescence Detection

2000 ◽  
Vol 83 (3) ◽  
pp. 698-713 ◽  
Author(s):  
Julie Fillion ◽  
François Sauvé ◽  
Jennifer Selwyn
Keyword(s):  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Fruits And Vegetables ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Detection Range

Abstract A method is described for the determination of 251 pesticide and degradation product residues in fruit and vegetable samples. Extraction of the sample with acetonitrile is followed by a saltingout step. Co-extractives are removed by passing a portion of the acetonitrile extract through an octadecyl (C18) solid-phase extraction cleanup cartridge and then, in a second cleanup, through a carbon cartridge coupled to an amino propyl cartridge. Determination is by gas chromatography with mass-selective detection in the selected-ion monitoring mode, and by liquid chromatography with post-column reaction and fluorescence detection for N-methyl carbamates. The method has been used for analysis of various fruits and vegetables, such as apple, banana, cabbage, carrot, cucumber, lettuce, orange, pear, pepper, and pineapple. Limits of detection range between 0.02 and 1.0 mg/kg for most compounds. Over 80% of the compounds have a limit of detection of ≤0.04 mg/kg.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

Simultaneous Analysis of Simple Coumarins and Furocoumarines in Cigarettes by Solid-Phase Extraction with Gas Chromatography-Mass Spectrometry

2017 ◽  
Vol 100 (5) ◽  
pp. 1559-1564 ◽  
Author(s):  
Yang Zheng ◽  
Xiuli Xu ◽  
Fei Yuan ◽  
Meiyi Yao ◽  
Shunli Ji ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Selected Ion Monitoring ◽  
Oasis Hlb ◽  
Coumarin 6

Abstract A sensitive, high-throughput analytical method based on a GC-MS method was established for the simultaneous quantitative determination of two categories of harmful coumarins: simple coumarins (coumarin, 6-methylcoumarin, 7-methoxycoumarin, 3,4-dihydrocoumarin, and 7-ethoxy-4-methylcoumarin) and furocoumarines (psoralen, 8-methoxypsoralen, 5-methoxypsoralen, and trioxysalen). The nine analytes were extracted with ethyl acetate, purified with Oasis HLB solid-phase extraction (SPE) cartridges, and identified and quantitatively determined by GC-MS in selected-ion monitoring mode. The LODs and LOQs of these compounds were in the ranges of 12.5–21.2 and 41.6–70.0 μg/kg, respectively. Average recoveries for the nine analytes ranged from 72.7 to 86.6% atLOQ, 1.5× LOQ, and 2× LOQ spike levels, with RSDs that were typically lower than 5.1%. TheSPE-GC-MS method developed in this study was initially applied to research coumarins in cigarette samples; it proved to be accurate, sensitive, convenient, and practical.

Detection of 30 Acidic Herbicides and Related Compounds as Their Pentafluorobenzylic Derivatives Using Gas Chromatography/Mass Spectrometry

1994 ◽  
Vol 77 (6) ◽  
pp. 1587-1604 ◽  
Author(s):  
Thomas Heberer ◽  
Susanne Butz ◽  
Hans-Juergen Stan
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Time Window ◽  
Solid Phase ◽  
Tap Water ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Acidic Herbicides ◽  
Related Compounds

Abstract Thirty phenoxyalkanoic acids, other acidic herbicides, and related compounds were derivatized with pentafluorobenzyl bromide to form their pentafluorobenzylic derivatives. Mass spectra are presented. Determination and detection of the derivatives was performed by capillary gas chromatography (GC)/mass spectrometry. With selected- ion monitoring, an optimized GC method, and appropriate time-window setting, the determination of all compounds could be achieved in a single GC run. The determination of ≤1 pg of the target compounds was achieved using electron-impact ionization in selected-ion monitoring mode. Most of the analytes were extracted from tap water, and recoveries were 80–100% when solid-phase extraction was applied with a carefully selected reversedphase-C18 adsorbent. The method enabled the detection of these contaminants from drinking water at the low nanogram-per-liter level when applying a concentration factor of 10 000.

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